Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof

A technology of zeolite molecular sieve and ZSM-5, which is applied in chemical instruments and methods, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminum silicate zeolite, etc., can solve the problem of high preparation cost, achieve convenient operation, reduce The effect of synthesis cost and good adsorption capacity

Inactive Publication Date: 2014-05-14
HUAINAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the deficiency that the preparation cost of ZSM-5 zeolite molecular sieve is high in the prior art, provide a kind of preparation method and application of low-cost ZSM-5 type zeolite molecular sieve; The present invention uses industrial waste fly ash as Raw material, tetrapropyl ammonium hydroxide (TPAOH) is template agent, extracts a large amount of Si, Al element transformation in the fly ash and prepares the ZSM-5 type zeolite molecular sieve that can be used directly, and the fly ash used in the present invention mainly The mineral crystal phase is quartz and mullite, and there is also an amorphous glass phase component. The content of Si and Al is relatively high, especially the ratio of Si / Al is high, and it has high comprehensive utilization value.

Method used

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  • Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof
  • Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof
  • Preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] With reference to the accompanying drawings, this embodiment of a low-cost ZSM-5 type zeolite molecular sieve preparation method, the fly ash used is from a thermal power plant in Huainan, the XRD ray diffraction pattern of the raw fly ash powder is shown figure 2 . The main mineral crystal phases of fly ash raw powder are quartz and mullite, as well as amorphous glass phase components. The main chemical components are analyzed by X-ray fluorescence spectrometer (XRF) in Table 1. It can be seen from Table 1 that Fe, Ca and other metal impurities in the fly ash used in this embodiment account for a part of the proportion, but the content of Si and Al is relatively high, especially with a relatively high Si / Al ratio. Silicon source and aluminum source have high comprehensive utilization value.

[0030] Table 1 The main chemical composition of fly ash (wt%)

[0031]

[0032] The chemical reagents used in this example are tetrapropylammonium hydroxide (TPAOH), NH 4 F, NaOH, H...

Embodiment 2

[0042] The preparation method of a low-cost ZSM-5 zeolite molecular sieve in this example is basically the same as that in Example 1. The preparation steps are briefly described as follows:

[0043] Dry the raw fly ash at 140°C for 20 hours to constant weight, mix the dry fly ash and the HCl solution with a mass percentage concentration of 10% at a solid-liquid ratio (g / mL) of 1:20, and stir thoroughly Centrifuge for 10 minutes at 5000 rpm for 30 min. After removing the supernatant, wash with deionized water to a pH of 6, and dry at 100°C for use.

[0044] Accurately weigh 20g of iron-removing fly ash and 44g of NaOH, grind uniformly to 400 mesh, then place it in a muffle furnace to melt for 3 hours at 500°C, after cooling, grind through a 200-mesh sieve, and then grind the resulting molten material. Add it to the deionized water at the ratio of solid-liquid mass ratio of 1:4, mix it into a slurry, and stir in a water bath at 80℃ for 24h to make the aluminosilicate in the fly ash i...

Embodiment 3

[0047] The preparation method of a low-cost ZSM-5 zeolite molecular sieve in this example is basically the same as that in Example 1. The preparation steps are briefly described as follows:

[0048] Dry the raw fly ash powder at 125°C for 22 hours to constant weight, mix the dry fly ash and HCl solution with a mass percentage concentration of 10% at a solid-liquid ratio (g / mL) of 1:20, and stir thoroughly Centrifuge for 13 minutes at 5000 rpm for 25 minutes, remove the supernatant, wash with deionized water to pH=7, and dry at 100°C for use.

[0049] Accurately weigh the iron-removing fly ash and NaOH according to the mass ratio m(SiO 2 ):m(NaOH)=1:2.2 ratio, grind uniformly to 200 mesh, then place it in a muffle furnace to melt at 450℃ for 4h. After cooling, grind through a 200-mesh sieve. The solid-liquid mass ratio of 1:3 is added to the deionized water, mixed into a slurry, and stirred in a water bath at 80℃ for 24 hours to make the aluminosilicate in the fly ash in OH - Dissol...

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Abstract

The invention discloses a preparation method of low-cost ZSM-5 type zeolite molecular sieve, and application of the low-cost ZSM-5 type zeolite molecular sieve, belonging to the field of a molecular sieve preparation technology. The method comprises the steps of a. drying pulverized fuel ash raw powder to constant weight, mixing HCl solution with the dried pulverized fuel ash, stirring, centrifuging, washing and drying for later use; b. grinding the pulverized fuel ash treated by the step a, mixing the ground pulverized fuel ash with NaOH for melting, cooling, grinding and screening by a molecular sieve; feeding the ground melt into deionized water, mixing, stirring under the condition of water bath, and carrying out centrifugal separation to obtain liquid supernatant; c. taking the liquid supernatant obtained in the step b, taking tetrapropylammonium hydroxide as a template agent and NH4F as a mineralizer, mixing and carrying out crystallization reaction; after that, taking out the product, quenching to the room temperature, washing, drying and roasting to obtain the zeolite molecular sieve. According to the method, the pulverized fuel ash discharged by a thermal power plant is fully utilized as a silicon-alumininm source and is used for replacing pure chemical reagents Si and Al for synthesizing the molecular sieve, so that the synthesis cost of the molecular sieve is lowered, and the utilization value is high.

Description

Technical field [0001] The invention relates to the technical field of molecular sieve preparation, and more specifically, to a method for preparing a ZSM-5 type zeolite molecular sieve by using fly ash discharged from a thermal power plant as the main source of silica and aluminum, and the application of the molecular sieve. Background technique [0002] ZSM-5 zeolite molecular sieve has very important applications in the field of catalysis and separation due to its unique shape-selective catalysis and acidic properties, and has always been a hot spot for chemical scientific researchers. At present, there have been a large number of reports on the preparation and performance research of ZSM-5 zeolite molecular sieve, but they mainly focus on using pure chemical reagents such as silica gel, water glass, silica sol, and tetraethyl orthosilicate as the source of silicon. In addition, aluminum sources such as aluminum nitrate and aluminum sulfate are added, and the preparation cost ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J20/18B01J20/30C02F1/28C02F1/62C02F101/22
Inventor 赵星郭红彦
Owner HUAINAN NORMAL UNIV
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